DESC:FORM 2

THE PATENTS ACT, 1970
(SECTION 39 OF 1970)
&
The Patents Rules, 2003

COMPLETE SPECIFICATION
(Section 10 and Rule 13)

INSECTICIDAL COMPOSITION OF FLONICAMID AND PROFENOFOS

We, COROMANDEL INTERNATIONAL LIMITED,
an Indian company incorporated under the Companies Act, 1956, and validly existing under the Companies Act, 2013. Having its registered office at Coromandel House, Sardar Patel Road, Secunderabad – 500 003, Telangana, India

The following specification particularly describes the invention, and the manner in which it is to be performed.
FIELD OF THE INVENTION
The present invention relates to a synergistic insecticidal composition comprising Flonicamid and Profenofos for controlling sucking pests. More particularly the invention provides insecticidal oil dispersion (OD) of Flonicamid and Profenofos with one or more suitable agrochemical auxiliaries, and a process thereof.

BACKGROUND OF THE INVENTION
In an agriculture-based economy, with inadequate resources, it is essential to resort to most economical and promising agricultural practices. It demands not only consistent efforts towards enhancing the crop yield but also efforts towards achieving fool proof protection and stability of crops against the attack of insects/pests and/or mites etc. with minimal or no side effects on the environment.

The protection of the crops and its produce from insect pests damage is an inherent requirement which is being addressed with the help of a vast range of insecticides and pesticides for over several decades now. Accordingly, in the presently existing agricultural practices, the use of organic chemicals and insecticides/pesticides have become almost inevitable as a curative or as precautionary measure.

It is desired to have insecticidal composition which is active against most or all type of potential insects i.e., a composition with contact / systemic as well as trans-laminar activity against the insects. This is also required to prevent the washing-out of sprayed insecticides due to rain or during irrigation.

Flonicamid is a systemic insecticide discovered by ISK. Flonicamid exhibits excellent performance for control of almost all important aphid species in apples, peaches, wheat, potato vegetables, cotton and ornamentals, etc. Flonicamid has no negative impact on pollinating insects or natural enemies, and thus, fl¬onicamid will provide a new option for integrated pest management programs. Flonicamid also has a good toxicological, environmental and ecotoxicological pro le.

Flonicamid chemically known as N-(Cyanomethyl)-4-(trifluoromethyl) pyridine-3-carboxamide and structurally represented as below:

Profenofos is a broad-spectrum organophosphorus pesticide, moderate toxicity, it is a kind of anticholinesterase, have tag, stomach poison function and interior absorption, be mainly used in the lepidoptera pest of control paddy rice, cotton and vegetable field, common insect such as cotton bollworm, beet armyworm, cabbage caterpillar, peach fruit borer etc. are had good control efficiency.

Profenofos chemically known as O-(4-Bromo-2-chlorophenyl) O-ethyl S-propyl phosphonothioate and having the structural formula as shown below:

WO 2002037964 A1 broadly discloses a combination of variable quantities of Flonicamid and one or more compounds, Profenofos for controlling insects or representatives of the order Acarina. This document discloses only emulsifiable concentrates, suspension concentrates, directly sprayable or dilutable solutions, spreadable pastes, dilute emulsions, sprayable powders, soluble powders, dispersible powders, wettable powders, dusts, granules. This document also discloses calcium or triethanolammonium salts of dodecylbenzenesulfonic acid as emulsifier; castor oil polyethylene glycol ether as surfactant.

CN 101669510 A discloses effective components of the composition contain Flonicamid and organophosphorus pesticide (Profenofos), wherein the preferred formulations are suspensions, water emulsions, microemulsions, water-dispersible granules, emulsifiable concentrates, wettable powders, and microcapsule suspensions for preventing and treating pests in plants. This document also discloses Profenofos complex preparation in Embodiment 10 comprising 1.02 grams of 97.6% Flonicamid,
11.11 grams of 90% Profenofos, calcium dodecyl benzene sulfonate 11.0 grams, Dimethyl formamide 10.2 grams and Toluene 100 grams.

CN 101946796 A discloses insecticidal composition comprising Flonicamid and Profenofos, wherein the composition can be prepared into emulsifiable oil, water emulsion, micro-emulsion, water dispersible granules and suspending agent for controlling sucking insects such as plant hopper, aphid, aleyrodid and leafhopper. No specific compositions of the combination are disclosed in this document.

None of the prior art disclosure describes oil dispersion composition of Flonicamid and Profenofos combination.

Accordingly, there is a need in the art to provide synergistic insecticidal oil dispersion compositions for controlling pests which are environmentally safer and stable product during storage.

It was surprisingly and unexpectedly found by the present inventors that a selective combination composition of comprising Flonicamid and Profenofos with one or more other agrochemical auxiliaries, possesses enhanced efficacy, improved penetration, and long duration control of phytopathogens as compared to its other traditional formulations with long storage stability across a wide temperature range and having no adverse impact on photosynthetic activity in plant and seed quality.

OBJECTIVE OF THE INVENTION
It is an objective of the present invention to provide a synergistic insecticidal composition of Flonicamid and Profenofos.

It is another objective of the present invention to provide an oil dispersion (OD) composition comprising of Flonicamid and Profenofos with one or more suitable agrochemical auxiliaries for controlling pests.

It is yet another objective of the present invention is to provide a process for the preparation of an oil dispersion (OD) composition comprising Flonicamid and Profenofos.

SUMMARY OF THE INVENTION
The present invention provides a synergistic insecticidal composition comprising Flonicamid and Profenofos.

In an aspect of the present invention provides an insecticidal comprising Flonicamid and Profenofos with one or more suitable agrochemical auxiliaries, wherein the suitable agrochemical auxiliaries are selected from the group comprising of a dispersing agent, an emulsifier, a rheology modifier, a wetting agent, an antifreezing agent, a disintegrating agent, a defoamer, a biocide, a viscosity agent, a base, a solvent, a base oil, and a filler.

In another aspect of the present invention provides an oil dispersion (OD) composition comprising of its active ingredients Flonicamid present in a range from 5% to 10% (w/w), Profenofos present in a range from 30% to 50% (w/w), and one or more suitable agrochemical auxiliaries present in a range from 50% to 80% (w/w), wherein the agrochemical auxiliaries are selected from the group comprising of a dispersing agent, an emulsifier, a rheology modifier, and a base oil.

In another aspect of the present invention provides an oil dispersion (OD) composition comprising:
a) Flonicamid in the range of 5% to 10% (w/w),
b) Profenofos in the range of 30% to 50% (w/w),
c) a dispersing agent in the range of 1% to 10% (w/w),
d) an emulsifier in the range of 1% to 5% (w/w),
e) a rheology modifier in the range of 1% to 2% (w/w), and
f) a base oil in the range of in the range of 30% to 50% (w/w).

In another aspect of the present invention provides an oil dispersion composition comprising:
a) Flonicamid in the range of 5% to 10% (w/w),
b) Profenofos in the range of 30% to 50% (w/w),
c) calcium dodecyl benzenesulfonate in the range of 2% to 5% (w/w),
d) castor oil based ethoxylate in the range of 5% to 10% (w/w),
e) fumed silica in the range of 1% to 2% (w/w), and
f) methyl soyate oil in the range of in the range of 40% to 50% (w/w).

In an embodiment of the present invention, a dispersing agent is selected from the group comprising of sodium lignosulphonates, sodium naphthalene formaldehyde condensates, ethoxylated C12-C16 alcohols, alkyl naphthalene sulfonate condensate, sodium salt of naphthalene sulfonate condensate, polymethyl methacrylate-polyethylene glycol graft copolymer, calcium dodecyl benzenesulfonate, and combination thereof, present in an amount of 1% to 10% (w/w).

In an embodiment of the present invention, an emulsifier is selected from the group comprising of ethoxylated and alkoxylated fatty acids, ethoxylated amines, ethoxylated alcohol, alkyl, and nonyl-phenol ethoxylates, ethoxylated sorbitan esters, castor oil ethoxylate and EO/PO copolymers, present in an amount of 1% to 5% (w/w).

In an embodiment of the present invention, a rheology modifier is selected from the group comprising of hydrophobic and hydrophilic fumed and precipitated silica particles, including fumed silica treated with a hexadecyl silane, and silicon dioxide, present in an amount of 1% to 2% (w/w).

In an embodiment of the present invention, a base oil is selected from the group comprising of methyl oleate, methyl soyate oil, methyl palmitate, and epoxidized soybean oil, present in an amount of 30% to 50% (w/w).

The present invention also provides a process for the preparation of an oil dispersion (OD) composition comprising the steps of:
a) blending all the active ingredients, rheology modifier, dispersing agent, and other agrochemical auxiliaries to high sheer dispersion at a temperature in the range of 30 to 50 oC,
b) milling the homogenized mixture to obtain particles of size in the range of 15-20 µ,
c) stirring the milled mixture, and cooling to room temperature,
d) collecting the sample.

DETAILED DESCRIPTION OF THE INVENTION
The following detailed description is presented to enable any person skilled in the art to make and use the invention. For purposes of explanation, specific nomenclature is set forth to provide a thorough understanding of the present application. However, it will be apparent to one skilled in the art that these specific details are not required to practice the invention. Descriptions of specific applications are provided only as representative examples. The present application is not intended to be limited to the embodiments shown but is to be accorded the widest possible scope consistent with the principles and features disclosed herein.

It is to be noted that, as used in the specification, the singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. Thus, for example, reference to a composition containing “a compound” includes a mixture of two or more compounds. It should also be noted that the term “or” is generally employed in its sense including “and/or” unless the content clearly dictates otherwise.

Similarly, the words "comprise", "comprises", and "comprising" are to be interpreted inclusively rather than exclusively. Likewise, the terms "include", "including" and "or" should all be construed to be inclusive, unless such a construction is clearly prohibited from the context. However, the embodiments provided by the present disclosure may lack any element that is not specifically disclosed herein. Thus, a disclosure of an embodiment defined using the term "comprising" is also a disclosure of embodiments "consisting essentially of” and "consisting of” the disclosed components. Where used herein, the term "example", particularly when followed by a listing of terms, is merely exemplary and illustrative and should not be deemed to be exclusive or comprehensive. Any embodiment disclosed herein can be combined with any other embodiment disclosed herein unless explicitly indicated otherwise.

The expression of various quantities in terms of “% w/w” or “%” means the percentage by weight, relative to the weight of the total solution or composition unless otherwise specified.

As used herein, the terms “insecticide” may be understood to include pesticides specifically used to destroy one or more species of insects.

As used herein, the term “synergistic composition” may be understood to include effective combination of more than one agrochemical that allows the application of the said agrochemical in a much lower dosage, which results in a less dosage treatment for the crops.

As used herein, the term “agrochemical auxiliaries” may be understood to include a range of surfactants, dispersing agents, organic or inorganic pigments, solvents, de-solvents, defoamers, and emulsions, crystallization inhibitors, viscosity modifiers, suspending agents, dyes, antioxidants, foaming agents, light absorbers, mixing aids, neutralizers or pH adjusting substances and buffers, corrosion inhibitors, fragrances, wetting agents, absorption enhancers, micronutrients, plasticizers, lubricants, thickeners, anti-freezing agents, sterilization agents among others.

In an embodiment of the present invention, an insecticidal composition comprises of Flonicamid and Profenofos with one or more suitable agrochemical auxiliaries.

The compositions of the present invention are formulated into various formulations such as a suspension concentrates (SC), an oil-based dispersions (OD), a suspoemulsion (SE), a water dispersible granule (WDG), water soluble powder (WP), and a granule (GR). Preferably, the insecticidal composition can be formulated as an oil dispersion (OD).

In another embodiment of the present invention, an oil dispersion (OD) composition comprising of its active ingredients Flonicamid present in a range from 5% to 10% (w/w), Profenofos present in a range from 30% to 50% (w/w), and one or more suitable agrochemical auxiliaries present in a range from 50% to 80% (w/w), wherein the agrochemical auxiliaries are selected from the group comprising of a dispersing agent, an emulsifier, a rheology modifier, and a base oil.

In another embodiment of the present invention, provides an oil dispersion (OD) composition comprising of:
a) Flonicamid in the range of 5% to 10% (w/w),
b) Profenofos in the range of 30% to 50% (w/w),
c) a dispersing agent in the range of 1% to 10% (w/w),
d) an emulsifier in the range of 1% to 5% (w/w),
e) a rheology modifier in the range of 1% to 2% (w/w), and
f) a base oil in the range of in the range of 30% to 50% (w/w).

As used herein, the term “dispersing agent” may be understood as a chemical substance, which is typically a surfactant, that is added to a suspension of solid or liquid particles in a liquid (such as a colloid or emulsion) to improve the separation of the particles and to prevent their settling or clumping. They can disperse active ingredients in the formulation and prevent agglomeration after dispersal in water.

Accordingly, the composition of the present invention contains a dispersing agent suitable for use in the present invention selected from the group comprising of sodium lignosulphonates, sodium naphthalene formaldehyde condensates, ethoxylated C12-C16 alcohols, alkyl naphthalene sulfonate condensate, sodium salt of naphthalene sulfonate condensate, polymethyl methacrylate-polyethylene glycol graft copolymer, calcium dodecyl benzenesulfonate, and combination thereof, present in an amount of 1% to 10% (w/w).

Accordingly, the composition of the present invention contains an emulsifier suitable for use in the present invention selected from the group comprising of ethoxylated and alkoxylated fatty acids, ethoxylated amines, ethoxylated alcohol, alkyl, and nonyl-phenol ethoxylates, ethoxylated sorbitan esters, castor oil ethoxylate and EO/PO copolymers, present in an amount of 1% to 5% (w/w).

Accordingly, the composition of the present invention contains a rheology modifier suitable for use in the present invention selected from the group comprising of hydrophobic and hydrophilic fumed and precipitated silica particles, including fumed silica treated with a hexadecyl silane, and silicon dioxide, present in an amount of 1% to 2% (w/w).

Accordingly, the composition of the present invention contains a base oil suitable for use in the present invention selected from the group comprising of methyl oleate, methyl soyate oil, methyl palmitate, and epoxidized soybean oil, present in an amount of 30% to 50% (w/w).

As used herein, the term “wetting agent” may be understood as a chemical substance which is typically a surfactant used to reduce the surface tension of the water by penetrating in between the water molecules and thus reducing the cohesion between them. The waxy surface of many insects, fungi and plants makes it difficult for most water-based pesticides solution to penetrate to their target. Hence, these wetting agents help the solution to spread on the leaf surface thus increasing their efficiency. These agents aid in the milling process.

Accordingly, the composition of the present invention contains a wetting agent suitable for use in the present invention selected from the group comprising of sodium isopropyl naphthalene sulfonate, fatty alcohol ethoxylate, and dispersant emulsifier blend.

As used herein, the term “anti-freezing agent” may be understood as a chemical substance which prevents the said formulation from freezing.

Accordingly, the composition of the present invention contains an antifreezing agent for use in the present invention selected from the group comprising of propylene glycol, and acrylate copolymer.

As used herein, the term “biocide” may be understood as a chemical substance used to destroy, deter, render harmless or exert a controlling effect on any harmful organism. The addition of these biocides to the agricultural formulations helps to prevent the possible growth of micro-organisms for longer duration.

Accordingly, the composition of the present invention contains a biocide for use in the present invention selected from the group comprising of 1,2-benzisothiazol-3(2H)-one and benzisothiazolin-3-one.

As used herein, the term “defoamer” may be understood as a chemical additive which is used to reduce and hinder the formation of foam in the liquid formulations.

Accordingly, the composition of the present invention contains a defoamer for use in the present invention selected from the group comprising of polydimethyl siloxane antifoam emulsion and polydimethyl siloxane.

As used herein, the term “viscosity modifier” may be understood as a chemical substance used to alter the viscosity or the thickness of a liquid. These are the substances that alter the fluid resistance to flow.

Accordingly, the composition of the present invention contains a viscosity modifier for use in the present invention selected from the group comprising of hydrated magnesium aluminosilicate and xanthan gum.

Accordingly, the composition of the present invention contains a solvent for use in the present invention are aromatic hydrocarbon (C9-10 aromatic hydrocarbons, solvent naphtha (petroleum) light aromatic, xylene, and toluene.

Accordingly, the composition of the present invention contains a disintegrating agent for use in the present invention is ammonium sulphate.

Accordingly, the composition of the present invention contains a filler for use in the present invention is maize starch (amylose and amylopectin).

Accordingly, the composition of the present invention contains a base suitable for use in the present invention is distilled water.

In yet another embodiment of the present invention, also provides a process for the preparation of an oil dispersion (OD) composition comprising the steps of:
a) blending all the active ingredients, rheology modifier, dispersing agent, and other agrochemical auxiliaries to high sheer dispersion at a temperature in the range of 30 to 50 oC,
b) milling the homogenized mixture to obtain particles of size in the range of 15-20 µ,
c) stirring the milled mixture, and cooling to room temperature, and
d) collecting the sample.

Preferably, the synergistic herbicidal composition can be formulated as an oil dispersion (OD), which is a stable suspension of active ingredient(s) in an organic fluid, which may contain other dissolved active ingredient(s), intended for dilution with water before use.

The oil dispersion (OD) composition of the present invention shows low gravitational separation without a substantial increase in viscosity (measured at a shear rate of 200). This could be achieved using low-density particles with a density equal or less than 0.27 g/cm3 that are importantly combined with a reduced amount of a rheological modifier such that the low-density particles balance the density from the dispersed particulates and that the rheological modifier is sufficient to hold the low-density particles within the suspension without increasing the viscosity to the level that would be required without low density particles.

The compositions of the present invention can be diluted with water or water solutions of agronomic compounds before use to produce a sprayable suspension composition which is used in treating plants or increasing plant growth, Dilution in water usually results in suspensions, emulsions, suspoemulsion or solutions of the agrochemical active ingredient at a concentration of at least 0.001 g/l.

A particular mode of administering the composition of the present invention is the administration to the aboveground parts of plants, to the leaves thereof (leaf-application). The number of applications and the administered doses are chosen in accordance with the biological and climatic conditions of life of the causative agent. The antifungal compositions though, can also be applied to the soil and get into the plants through the root system (systemic activity) in case the locus of the plants is sprayed with a liquid composition or if the components are added to the soil in a solid formulation e.g., in the form of granulate (soil application).

When using the active compound combinations according to the invention, the application rate can be varied within a relatively wide range, depending on the kind of application. For the treatment of parts of plants, the active-compound combination application rates are generally between 0.1 and 10000 g/ha, preferably between 100 and 2500 g/ha. For seed dressing, the active compound combination application rates are generally between 0.001 and 50 g per kilogram of seed, preferably between 0.01 and 20 g per kilogram of seed. For the treatment of the soil, the active-compound combination application rates are generally between 0.1 and 10000 g/ha preferably between 1 and 5000 g/ha.

The following examples describe the nature of the invention which are given only for the purpose of illustrating the present invention in more detail and are not limitative and relate to solutions, which have been particularly effective on bench scale.

EXAMPLES:
Example-1: Composition of Flonicamid 7% + Profenofos 40% oil-dispersion (OD)
S. No. Composition Function %(w/w)
1. Flonicamid@ 94 % Insecticide 7.0
2. Profenofos @95 % Insecticide 40.0
3. Calcium dodecyl benzenesulfonate Dispersing agent 3.0
4. Castor oil based ethoxylate Emulsifier 5.0
5. Fumed silica (after treated with hexadecyl silane) Rheology modifier 1.0
6. Methyl soyate oil Base oil 44.0
Total 100

Manufacturing Process:
Flonicamid and Profenofos were dissolved in methyl soyate oil and to this mixture was added fumed silica. To this was added Calcium dodecyl benzenesulfonate followed by castor oil ethoxylate. The sample was milled at 25 °C and particle size is maintained at < 5µ. The sample is checked for quality analysis and packed in HDPE drum.

Example-2: Composition of Flonicamid 7% + Profenofos 40% Wettable Powder (WP)
S. No. Composition Function %(w/w)
1. Flonicamid@ 94% Insecticide 7.0
2. Profenofos @95% Insecticide 40.0
3. Sodium isopropyl naphthalene sulfonate Wetting agent 2.5
4. Alkyl naphthalene sulfonate condensate Dispersing agent 5.0
5. Sodium lignosulphonate Dispersing agent 4.0
6. Silicon dioxide (ppt Silica) Rheology modifier 1.0
7. Maize starch (amylose and amylopectin) Filler 40.5
Total 100

Manufacturing Process:
Flonicamid and Profenofos, sodium isopropyl naphthalene sulfonate, alkyl naphthalene sulfonate condensate, sodium lignosulphonate, silicon dioxide and maize starch were blended in a ribbon blender for 15 minutes. This was followed by milling the sample through air jet milling instrument (Inlet pressure - 4kg/cm2 and Grinding pressure - 6kg/ cm2 for milling the sample) and collecting the material and packing (the particle size distribution (PSD) of the milled material should be <10 µ).

Example-3: Composition of Flonicamid 7% + Profenofos 40% Water dispersible granules (WDG)
S. No. Composition Function %(w/w)
1. Flonicamid@94% Insecticide 7.0
2. Profenofos @95% Insecticide 40.0
3. Sodium isopropyl naphthalene sulfonate Wetting agent 2.5
4. Alkyl naphthalene sulfonate condensate Dispersing agent 5.0
5. Sodium lignosulphonate Dispersing agent 4.0
6. Ammonium sulphate Disintegrating agent 1.0
7. Maize starch (amylose and amylopectin) Filler 40.5
Total 100

Manufacturing process:
Flonicamid and Profenofos technical, sodium isopropyl naphthalene sulfonate, alkyl naphthalene sulfonate condensate, sodium lignosulphonate, ammonium sulphate and maize starch were blended in a pre-blender and mixing it for 1 hr. This was followed by milling the sample through air jet mill instrument at Inlet pressure 2-3 kg/cm2 and grinding pressure 6 kg/ cm2 and checking the particle size < 12 micron. The milled material was collected and post blended for 1 hr. This was followed by extruding the granules 35 at rpm (1.0 mesh). The granules were collected and dried the sample at 45 °C for 30 min. The sample was checked for quality analysis and formulated in suitable packaging.

Example-4: Composition of Flonicamid 7% + Profenofos 40% Suspension Concentrate (SC)
S. No. Composition Function %(w/w)
1. Flonicamid@94% Insecticide 7.0
2. Profenofos @95% Insecticide 40.0
3. Fatty alcohol ethoxylate Wetting agent 1.5
4. Polymethyl methacrylate-polyethylene glycol graft copolymer. Dispersing agent 2.0
5. Propylene glycol Antifreezing agent 10.0
6. 1,2-Benzisothiazol-3(2H)-one Biocide 0.1
7. Polydimethylsiloxane antifoam emulsion Defoamer 0.5
8. Xanthan gum Viscosity Modifier 5.0
9. Methyl soyate oil Base oil 33.9
Total 100

Manufacturing process:
In a pre-mixer, vessel no.1 the fatty alcohol ethoxylate, polymethyl methacrylate-polyethylene glycol graft copolymer was added. After 15 min 1,2-benzisothiazol-3(2H)-one followed by 0.5 parts of polydimethylsiloxane antifoam emulsion were added. The mixture was stirred for 15 mins by adding water followed by the addition of Flonicamid and Profenofos. The mixture was stirred for homogenization. The wet slurry from the above vessel was passed through dyno-mill at a temperature below 30°C and material was collected in another vessel no.2 (post mixer). Continuous stirring was maintained in both the vessels to avoid sedimentation. The particle size distribution 10 (PSD) of the sample was checked. The PSD of the material should be d90 < 15 µ. If the d90 is higher than > 15 µ then the mixture was grinded till the PSD value complies with the specification. The required quantity of xanthan gum was added to the wet slurry in vessel no.2 and stirred for 3 hrs. for homogenization. The sample was checked for complete analysis and packed in designated bottles.

Example-5: Composition of Flonicamid 7% + Profenofos 40% Suspoemulsion (SE)
S. No. Composition Function %(w/w)
1. Flonicamid@94% Insecticide 7.0
2. Profenofos @95% Insecticide 40.0
3. Aromatic hydrocarbon (Solvent C9) solvent 10.0
4. Propylene glycol Antifreezing agent 5.0
5. Ethoxylated C12-16 alcohols Dispersing agent 2.0
6. Dispersant emulsifier blend Wetting agent 2.0
7. Benzisothiazolin-3-one Biocide 0.07
8. Polydimethylsiloxane Defoamer 0.5
9. Sodium naphthalene condensate formaldehyde Dispersing agent 2.0
10. Castor oil ethoxylate Emulsifier 2.0
11. Xanthan gum Viscosity Modifier 2.0
12. Water Base 27.43
Total 100

Manufacturing process:
Propylene glycol and sodium naphthalene condensate formaldehyde, ethoxylated alcohols C12-16, water and 1,2- benzisothiazolin-3-one, and polydimethylsiloxane were added by stirring. Mixture was stirred for 15 minutes and Flonicamid technical and dispersant emulsifier blend was added. The mixture was homogenized. The organic phase was prepared by adding sodium naphthalene condensate formaldehyde heated in a vessel to 40°C. and Profenofos by slow stirring. Castor oil ethoxylate was added and stirred for 30 mins. Both the aqueous and organic phases were mixed with stirring. Wet slurry was passed through dyno-mill at temperature less than 35° C and collected in separate vessel. Continuous stirring was maintained in vessels to avoid sedimentation. Sample was analysed to check the particle size distribution (PSD). Milling process was repeated till desired particle size was obtained (i.e., d90 < 15 µ). In the next step xanthan gum was added in propylene glycol then benzisothiazolin-3-one was added to this slurry into distilled water and stirred the mixture until it gets lumps free homogeneous mixture. This gel was kept for 4-5 hours to get a translucent homogeneous gel. The required quantity of gel was added to the wet slurry prepared above and stirred the mixture for ~3 h for homogenization. Material was packed in a suitable bottle.

Efficacy study for combination of Flonicamid 7% + Profenofos 40% OD:

Field and Synergy Studies: Cotton

Cotton (Gossypium hirsutum L.) is the most important cash crop in India with an expanse of 11-12 million hector area under cultivation. It grows well in almost all areas of the country however, mainly grown in nine states major cotton growing states which includes Punjab, Haryana, Rajasthan in North India, Maharashtra, Gujarat & Madhya Pradesh in Central India, and Tamilnadu, Karnataka, Andhra Pradesh & Telangana in South India.

The field efficacy trials were conducted in cotton on cotton sucking pest complex. The sucking pests viz., Leafhopper, Amrasca biguttula biguttula (Ishida), Aphid, Aphis gossypii (Glover), and Thrip, Thrips tabaci (Linnman) cause severe damage and serious threat to many field crops at early stage and can also affect the crop stand and yield.

Trials were conducted to evaluate the efficacy of innovative mixtures of Flonicamid and Profenofos. Trials were conducted with randomized block design with net plot size of 5m x 6m. Cotton crop was raised with all standard agronomic practices. Spraying was done with manual operated backpack sprayer with 500 liter of water spray volume per hectare at 45-50 days after sowing. The observations were recorded by counting the number of sucking insects (Jassids, Thrips & Aphids) per leaf, six leaves per plant and five plants per plot.

The observations were recorded at before spraying, 10 DAA (Days after application). The percent insect control was worked out by below formula:
Number of insects in treated plot
% Insect Control = --------------------------------------------- x 100
Number of insects in untreated plot

After calculating % Insect control, the synergistic pesticidal action of the inventive mixtures calculated by Colby’s formula as follows:

Appropriate analysis of plant response to herbicide combination is critical in determining the type of activity observed. The most widely used model is one Gowing* derived and Colby** modified. Gowing described a mathematical formula for calculating the predicting response values for pesticide mixtures. He suggested the expected (E) percent inhibition of growth induced by pesticide A plus pesticide B is as follows, *(Jerry Flint et al, 1988) ***

If A1 = the percent inhibition of growth by pesticide A at given rate
B1 = the percent inhibition of growth by pesticide B at given rate then,
B1 (100 – A1)
E = A1 +
100
When the percentage of pesticidal control observed for the combination is greater than the expected percentage, there is a synergistic effect. (Ratio of O/E > 1, means synergism observed.)

Reference:
*Gowing, D. P. 1960. Comments on tests of herbicide mixtures. Weeds 8:379–391.
**Colby, S. R. 1967. Calculating synergistic and antagonistic responses of herbicide combinations. Weeds 15:20–22
*** Jerry Flint et al, 1988. Analyzing Herbicide Interactions: A Statistical Treatment of Colby's Method. Weed Technology 2: 304-309

Table 1: Sucking Pests control in Cotton:

Compositions
Dose Gram Active/hectare % Insect Control at 10 DAA
Jassids Thrips Aphids
Flonicamid 50 % WG 67.5 85.5 26.8 85.1
Profenofos 50 % EC 450 27.5 80.5 26.2
Flonicamid 7% + Profenofos 40% OD
67.5 + 450
92.8
94.6
95.2
OD – Oil dispersion, WG-Wettable Granules, EC-Emulsifiable Concentrate, DAA- Days After Application.

Table 2: Sucking Pests control in Cotton:

Active Dose (GAH)
Jassids
Thrips
Aphids
Expected Actual Expected Actual Expected Actual
Flonicamid 50 % WG 67.5
-- 85.5
-- 26.8
-- 85.1
Profenofos 50 % EC 450
-- 27.5
-- 80.5
-- 26.2
Flonicamid 7% + Profenofos 40% OD 67.5+450 61.3 92.8 63.9 94.6 64.3 95.2
Ratio of O/E 1.51 1.48 1.38

Table 1 & Table 2, Trial results show excellent efficacy of Flonicamid + Profenofos combination insecticide against sucking pests Jassids, Thrips & Aphids. ,CLAIMS:WE CLAIM:

1. An insecticidal oil dispersion composition for controlling pests, which comprising
a) Flonicamid present in a range from 5% to 10% (w/w),
b) Profenofos present in a range from 30% to 50% (w/w), and
c) one or more suitable agrochemical auxiliaries present in a range from 50% to 80% (w/w).

2. The insecticidal oil dispersion composition as claimed in claim 1, wherein the composition is comprising of:
a) Flonicamid in the range of 5% to 10% (w/w),
b) Profenofos in the range of 30% to 50% (w/w),
c) a dispersing agent in the range of 1% to 10% (w/w),
d) an emulsifier in the range of 1% to 5% (w/w),
e) a rheology modifier in the range of 1% to 2% (w/w), and
f) a base oil in the range of in the range of 30% to 50% (w/w).

3. The composition as claimed in claim 2, wherein the dispersing agent is selected from the group comprising of sodium lignosulphonates, sodium naphthalene formaldehyde condensates, ethoxylated C12-C16 alcohols, alkyl naphthalene sulfonate condensate, sodium salt of naphthalene sulfonate condensate, polymethyl methacrylate-polyethylene glycol graft copolymer, calcium dodecyl benzenesulfonate, and combination thereof.

4. The composition as claimed in claim 2, wherein the emulsifier is selected from the group comprising of ethoxylated and alkoxylated fatty acids, ethoxylated amines, ethoxylated alcohol, alkyl, and nonyl-phenol ethoxylates, ethoxylated sorbitan esters, castor oil ethoxylate and EO/PO copolymers.

5. The composition as claimed in claim 2, wherein the rheology modifier is selected from the group comprising of hydrophobic and hydrophilic fumed and precipitated silica particles, including fumed silica treated with a hexadecyl silane, and silicon dioxide.

6. The composition as claimed in claim 2, wherein the base oil is selected from the group comprising of methyl oleate, methyl soyate oil, methyl palmitate, and epoxidized soybean oil.

7. The composition as claimed in any of the claims 1 to 6, for controlling pests is applied to the pests or their environment.

8. The process for the preparation of an oil dispersion (OD) composition as claimed in claim 1, wherein the process comprising the steps of:
a) blending all the active ingredients, rheology modifier, dispersing agent, and other agrochemical auxiliaries to high sheer dispersion at a temperature in the range of 30 to 50 oC,
b) milling the homogenized mixture to obtain particles of size in the range of 15-20 µ, stirring the milled mixture, and cooling to room temperature, and
c) collecting the sample.

Dated this Seventh (7th) day of September, 2023

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Dr. S. Padmaja
Agent for the Applicant
IN/PA/883